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Applications of Profile Analysis for Micro-Crystalline Properties From Total Pattern Fitting

Published online by Cambridge University Press:  06 March 2019

Daniel Louër
Daniel Louër*
Affiliation:
Laboratoire de Cristallochimie (URA CNRS 1495), Université de Rennes Avenue du Général Leclerc, 35042 Rennes cedex, France
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Extract

The characterization of finely divided and structurally imperfect solids is required in the study of many classes of materials, e.g. ceramics, catalysts, decomposition products. Diffraction line broadening is influenced by the microstructure of the solid and is a valuable technique for a unique characterization of a material in terms of size and morphology of crystallites (a region over which diffraction is coherent) and imperfections (microstrains, d- spacing fluctuations, stacking faults, etc). The extraction of these features has traditionally been based on the study of individual diffraction lines, which restricts the analysis to a limited number of directions of diffraction vectors. The complexity of most powder patterns has been a serious impediment to the widespread use of the procedure for detailed microstructural characterization. The advent of fitting techniques, with the use of structural information (Rietveld method) and without structure model (pattern decomposition method) have extended the frontiers of diffraction line profile analyses. In the Rietveld method it has been recommended to have a prior knowledge of the origin and lattice direction dependences of the imperfection effect before embarking in the modelling of line broadening through the pattern. This modelling can be carried out with pattern decomposition methods, which provide individual diffraction lines for a subsequent study of microstructural properties. Several aspects of this technique, performances, limitations and practical problems are reviewed and discussed. Applications to oxides with high specific surface-area are used to illustrate the detailed microstructural information contained in a powder diffraction pattern.

Type
Research Article
Information
Advances in X-Ray Analysis , Volume 37: Forty-Second Annual Conference on Applications of X-ray Analysis, August 2-6, 1993 , 1993 , pp. 27 - 35
Copyright
Copyright © International Centre for Diffraction Data 1993

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References

1. Delhez, R., de Keijser, T.H., Langford, J.I., Louer, D., Mittemeijer, E.J. and Sonneveld, E.J., Chapter 8, in: The Rietveld Method, R.A. Young, ed., Oxford Univ. Press (1993).Google Scholar
2. Enzo, S., Polizzi, S. and Benedetti, A., Zeits. Krist. 170:275 (1985).Google Scholar
3. Niepce, J.C. and Benabad-Sidky, A., Chemica Scripta 26A:11 (1986).Google Scholar
4. Toraya, H., Yoshimura, M. and Somiya, S., J. Appl. Cryst. 16: 653 (1983).Google Scholar
5. Le Bail, A. and Louer, D., J. Appl. Cryst. 11:50 (1978).Google Scholar
6. Langford, J.I., Louer, D., Sonneveld, E.J. and Visser, J.W., Powder Diff. 1:211 (1986).Google Scholar
7. Toraya, H., J. Appl. Cryst. 19:440 (1986).Google Scholar
8. Toraya, H., Powder Diff. 4:130 (1989).Google Scholar
9. Langford, J.I., J. Appl. Cryst. 11:10 (1978).Google Scholar
10. Langford, J.I., m:Accuracy in Powder Diffraction II, E. Prince & J.K. Stalick, ed., NISTSpec. Publ. 846, pp. 110 126 (1992).Google Scholar
11. Louer, D. and Langford, J.I., J. Appl Cryst. 21:430 (1988).Google Scholar
12. Wilson, A.J.C., X-ray Optics, 2nd ed. London: Methuen (1962).Google Scholar
13. Niepce, J.C., Mesnier, M.T. and Louer, D., J. Solid State Chem. 22:341 (1977).Google Scholar
14. Louer, D., Weigel, D. and Langford, J.I., J. Appl Cryst. 5:353 (1972).Google Scholar
15. Louer, P., Auffredic, J.P., Langford, J.I., Ciosraak, D. and Niepce, J.C., J. Appl. Cryst. 16:183(1983).Google Scholar
16. Louer, D., Vargas, R. and Auffredic, J.P., J. Am. Ceram. Soc. 61: 136 (1984).Google Scholar
17. Langford, J.I. and Louer, D., J. Appl. Cryst. 15:20 (1982).Google Scholar
18. Plevert, J. and Louer, D., J. Chim. Phys. 87:1427 (1990).Google Scholar
19. Langford, J.J. and Louer, D., J. Appl Cr,'st. 24:149 (1991).Google Scholar
20. Langford, J.I., Boultif, A., Auffredic, J.R and Louer, D., J. Appl. Cryst. 26:22 (1993).Google Scholar
21. Toraya, H., J Appl Cryst. 18:351 (1985).Google Scholar
22. Pelloquin, D., Louer, M. and Louer, D., J. Solid State Chem., in press.Google Scholar
23. Haider, N.C. and Wagner, C.N.J., Acta Oyst. 20:312 (1966).Google Scholar